Delustring and weighting textile materials



- PotentedMar. 4, 1947 DELUSTRING AND WEIGHTING TEXTILE MATERIALSRobinson Percy Foulds and John Thompson Marsh,

Manchester, England, assignors to Tootal Broadhurst Lee Company Limited,Manchester, England, a British company No Drawing. Application October11, 1941, Serial No. 414,680. In Great Britain September 12,

'7 Claims. i

This invention relates to improvements in the treatment of fibres, yarnsor fabrics, particularly for delustrlng natural silk, artificial silk ofall types including cellulose esters or ethers or regenerated cellulosesuch as viscose silk, and has for its object to provide a new orimproved process for treating such material or for weighting and/ordelustring natural, silk, linen or other materials.

Further objects of the invention are to avoid waste of reagents, toimprove control, to allow higher concentrations of reagents to beemployed and to obtain pattern eifects of a very varied character.

The invention is a continuation in part of our application No. 93,232.

According to the present invention, the textile material is treated withthe ingredients in two phases or stages. 1. e., with some of theingredients in one fluid, either liquid or gaseous, and with theremaining ingredients in another fluid. Illustrative of a desirable twophase procedure, two diiferent liquid baths may be employed forsuccessive treatment of the textile material. One bath may contain asolution of two of the ingredients and a second bath the third, but ifdesired the first bath may contain some proportion of all theingredients and the second bath the requisite proportion of on or moreof them to effect rapid precipitation.-

The main advantages are as follows:

(a) If, for instance, the cloth or yarn is first passed through a bathcontaining urea, then there is obviously no waste of urea. as the bathcan be exhausted. In the case of the one-bath process there will alwaysbe a certain amount of methylene urea precipitate which cannot be used.Our experience-has been that it is not possible to exhaust the reagentsin a one-bath process, whether it be composed of the simple solutionwhich we employ or the more complicated solutions obtained by dissolvingsolid partial condensates in acid.

(b) Another advantage of the two-bath process lies in the greatercontrol which may be exercised. Once the methylene urea starts formingin the one-bath process there is very little which can be done to hinderit and the deposition takes place fairly rapidly. In the twobath processgreater control is possible as it is only in the second bath that anyprecipitation is likely to occur and this second bath, usually offormaldehyde, may be kept to such dimensions that renewal of the liquoris necessary before precipitation occurs in the bath.

The use of two baths enables many variations to be made in theconcentrations of the reagents in the baths and so permits of a greaterrange of delustring eflects.

The precipitation of methylene urea is to some extent a time reactionand this is capable of more exact control in the case of the two-bathprocess.

(0) For certain effects, mainly localised effects. where contrast isessential, the amount of urea is critical in many cases and this isanother point in favour of the two-bath process. For instance, in someeflects it is necessary to have 14% of urea in the cloth and we have notfound a satisfactory means of achieving this by any one-bath process.

(11) Where a heavy matt effect is necessary, as against a mereopalescence, it is practically impossible to obtain this by a one-bathprocess on a commercial scale; this is important where strong contrastsare required. Similar considerations apply where methylene urea is usedfor increasing the weight and bulk of the cloth, here again the two-bathprocess is preferable.

(e) Lastly, the range of pattern eflects (coloured, lustrous pattern ona white matt ground and many variations on this idea) is obviously verylimited in the one-bath process.

In the two-bath process it is possible to impregnate with the urea sayand then apply the printing technique, plain resists, coloured resists,etc., before treating in the second bath which produces the local matteffect where desired. This offers much more scope for the contrast ofmatt 1 components thereof and then bringing about precipitation of aninsoluble product from the solution. The material is impregnated withthe solution containing a precipitant in sufiicient quantity to form onthe textile material, after sulficient time of contact, a precipitatesubstantially fast to washing. The material impregnated with thesolution may alternatively be brought into contact with a precipitantsuch as an acid. Alternatively the material may be first treated with aprecipitant such as an acid and then impregnated with theurea-formaldehyde solution.

The textile material may be treated with the components of a syntheticcondensation product, separately and in any desired sequence, but it ispreferred to impregnate with urea and formaldehyde simultaneously.

When yarns or fibres are treated, the impregnation is performed withoutmaterially distorting the materials.

Where weighting is required, it is desirable to bring about theprecipitation on Or in the material of a large amount of insolublecondensation product. For delustring alone. smaller quantities willsuffice.

Fibres, yarns or fabrics may be treated by the process and the materialso treated will withstand washing without regaining its lustre. Thetreated materials can be dyed. Cellulosic materials treated by thepresent process will, withstand the mercerisation operation, and'canalso be dyed with acid dyes.

Example 1 Urea I m 60 Formaldehyde (neutral 40% solution) cc 100 Waterems 100 j 3 Example 2 Urea gms Formaldehyde (neutral 40% solution) cc100 Water gms 100 are mixed together without any heating, and thefabric, yarn or fibre in the form of silver or roving' well wetted witha solution, squeezed and then subjected to acid vapour until thedelustring has occurred, then well washed'with soap and soda ashsolution together with an oil, and finally washed and dried as inExample 1.

Example 3 Urea gms-- 100 Formaldehyde (neutral 40% solution) cc 200 arerefluxed with 3% 'NHiOH (sp. gr. .880) for 3 mins. at the boil, cooled,300 cc. water added and acidified with /2 to 1% tartaric acid. Fabric,yarns or fibres are immersed in this solution passed' through a mangleand :allowed to stand until the delustring'has taken place, and finallywashed and dried as in Example 1.

Example 4 60 gms. urea are dissolved in 100 s, 0 maldehyde (solution40%). A natural silk fabric is run through this solution and squeezedthrough rollers to ensure even penetration. The cloth is then passedquickly through 4% hydrochloric acid (spec. grav. 1.02) and the reactionallowed to proceed until precipitation takes place. The amount ofweighting obtained will depend on the amount of liquor left on thecloth, on the nature of the cloth to be treated, on the time for whichprecipitation is allowed to take place and on the nature of thecatalyst. After precipitation has taken place the fabric is well washedwith soap and soda ash and oil, then washed in water and finally dried.

In order to obtain further increase in weight, the whole process canthen be repeatedly performed until the. requisite increase in weight isobtained.

It is also possible to obtain plain (undyed) or dyed pattern efiects byapplying the process to selected areas of the yarn or fabric in any ofthe ways well known for producing patterns, e. g., the suitablythickened urea-formaldehyde solution may be applied by direct printingfollowed by precipitation; selected areas may be treated with a suitableresist (e. g., with the ethanolamines and other bases or with knownresists and then the delustring process applied, or selected areas ofthe delustred material may have the lustre restored by discharging(printing with a thickened acid) and steaming, followed by washing). Thepatterned fabric may be dyed or dyes may be incorporated in the resist.

Example 5 oured efiects can thus be obtained on a matt ground.

Example 6.-- 4ll-over delustred efiect 25 lbs. of urea was dissolved in10 gals. of water and 3 qts. of glycerine added. An all-viscose satincloth was impregnated with this solution and excess liquid squeezed offby passing it between the bowls of a two-bowl mangle adjusted so as toleave a quantity of liquor on the cloth equivalent to about of its ownweight.

The cloth was then dried at a moderate temperature and then impregnatedwith a solution of 60 parts by volume of commercial 40% formaldehyde and4 parts by volume of sulphuric acid (specific gravity 1.72) in 40 partsby volume of water. The cloth was then allowed to stand exposed to theair for 6-7 mins. to allow the delustring effect to develop, after whichtime the cloth was Washed first in water, then in soap solution andfinally rinsed in water and dried.

Example 7.Delustred coloured design with an undelustred background Therequisite amount of vat dye ester, for example, Soledon or Indigosoldyestufis, is dissolved in one part by volume of water or other solvent.This mixture is added to 9 parts by volume of a paste made by mixinglbs. urea, 8 lbs. sodium chlorate, 6 lbs. ammonium chloride, 3 ozs.

aciaeeo 8 ammonium vanadate, 4 gals. glycerine, 23 gals. um dragon orwater to dissolve the above chemicals, 1 qt. ammonia, and the whole thenmade up to 36 gallons.

A cotton viscose mixture fabric was printed with this colour, dried at amoderate temperature and passed through an ager fora-5 mins. to developthe colour. The fabric was then impregnated with a cold solutioncontaining 65 parts by volume of commercial 40% formaldehyde, 5 parts byvolume of sulphuric acid (specific gravity 1.72) and 30 parts by volumeof water and then passed face downwards through a two-bowl mangle.

The cloth was then allowed to stand exposed to the air for 6-7-mins.during which time the delustering effect developed. The fabric was thenwashed in water and again in dilute soda ash solution and finally washedin boiling soap solution. The fabric was then rinsed in water andfinished in the usual way.

Components of synthetic condensation products other than those indicatedmay be used but those which will react rapidly in presence of a catalystsuch as an acid are particularly suitable. The process differs from thatdisclosed in German Patent 499,818 in that precipitation of an insolublecondensation product is designedly brought about to make resin formationdimcultz it is not necessary to dry the material and heat it to a hightemperature since the intermediate compound can be made insoluble whilethe fabric is in the wet stateby the action of acid at room temperature.As the product is not deposited in a coherent impermeable layer butrather in particulate form, it is possible to treat a textile materialto delustre it, and then to treat it further according to the process ofGerman Patent 499,818 to improve its resistance to creasing, or to dyeit, or to submit it to other suitable textile processes. j

The treatment is effected in such manner as to cause a large reductionof lustre.

The lustre of a fabric is due to the specular reflection (i. e.,reflection as from a mirror) of light from the fibres.

For the purpose of measurement it may be defined as the ratio of theintensity of the specularly reflected beam at a given angle to thediffusely reflected beam in any direction.

It is assumed that the difl'usely reflected beam is of the sameintensity in all directions.

As lustre defined in this way varies with the direction in which thefabric is viewed. we prefer to make all measurements in the direction ofmaximum lustre.

In the special example of an all-viscose satin we wish to definedelustring as reducing the lustre at least to /3 the original lustre.With less lustrous fabrics than all-viscose satin, not so great a.reduction is obtained with similar treatment; in treating other kinds offabrics the treatment should be such as if applied to an all-viscosesatin, its lustre would be reduced at least to Va the original lustre.

The treatment should not be such as to deposit a coherent resinouslayer. The time of treatment must be sufliciently prolonged to allow ofadequate precipitation, though this varies with acidity, dilution,temperature and ratio of formdrying the same. to remove therefrom'anysubstance or ingredient adapted to cause resin formation upon the dryingof said material. Illustratively, this may be accomplished by washingthe fabric with an aqueous solution pursuant to the various exampleshereinabove disclosed.

We declare that what we claim is:

1. A process for delustring textile material in aqueous solution whichcomprises impregnating said material with a solution containing urea andcontacting the so treated material in another phase with anothersolution containing an aldehyde and an acid, whereby an insoluble,nonresinous, synthetic condensation product in particulate form isprecipitated in situ on the material to delustre the same, and washingsaid wet textile material having the non-resinous product precipitatedthereon to remove any ingredient adapted to cause resin formation upondrying said material.

2. The method as in claim 1 wherein the aldehyde is formaldehyde and theacid is hydrochloric acid.

3. A process for delustring textile material 1 which comprisesimpregnating said material with an aqueous solution containing urea,drying, printing with an acid-resisting agent, and contacting the sotreated material in another phase with another aqueous solutioncontaining an aldehyde and an acid, whereby an insoluble, nonresinous,synthetic condensation product in particulate form is precipitated insitu on the material to delustre the same, and washing the wet textilematerial with substances adapted to substantially completely remove anyum'eacted ingredients prior to drying the same.

4. The process of delustring textile material by the method ofprecipitating an insoluble nonresinous material by addition of an acidto a solution providing a source of amino and aldehyde compounds capableof forming an aminoplastic aldehyde resin on condensation and adapted toform a non-resinous compound in aqueous solution characterized by thefeature I that the textile material is contacted in at least two phaseswith at least two diflferent ingredients including an amino compound, analdehyde and an acid, each phase containing at least one and less thanall of said reagents, the two phases jointly including all of saidingredients and water, and contacting said wet textile material havingthe non-resinous precipitate thereon with an aqueous liquid adapted toremove any substance which will cause resin formation upon drying said88 material.

5. The process of delustring textile material with metylene ureacharacterized by the feature that the material is treated in twodifferent baths with two different solutions jointly containing urea,formaldehyde, water and sufl'lcient acid so that on interaction of saidsolutions methylene urea is precipitated in situ on the textilematerial, and washing the wet textile material after said methylene ureaformation with an alkaline solution, to thereby revent resin formationupon drying said material.

6. The process of delustring textile material by the precipitationthereon of a water insoluble non-resinous substance comprising treatingthe textile material in two distinct phases which jointly include anaqueous solution containing as ingredients urea and formaldehydetogether with an acid in quantity suillcient to cause the precipitationof methylene urea, each phase con- 16 taining at least one and less thanall of said in- 'quantity sufl'lcient to cause the precipitation of saidnon-resinous substance, each phase containing at least one and'less thanall of said ingredients, thereby forming said non-resinous precipitatein situ on said textile materiaL- and removing from said wet textilematerial having said precipitate thereon any substance adapted to causeresin formation upon drying the said material.

ROBINSON PERCY FOULDS. JOHN THOMPSON MARSH.

REFERENCES CITED The following references are of record in the 5 file ofthis patent:

UNITED STATES PATENTS Number 10 1,734,516 1,925,914 2,261,556 2,302,7782,302,779

Number 346,793

Name Date Foulds Nov. 5, 1926 Lanker Sept. 5, 1933 Marsh Nov. 4, 1941Landolt et al. (1) Nov. 24, 1942 Landolt et a1. (2) Nov. 24, 1942 RivatJuly 5, 1938 FOREIGN PATENTS Country Date British Apr. 17, 1931 BritishJune 14, 1937 British Jan. 16, 1939

